CN107934997A - A kind of method using core grade ZrO 2 production waste discharge production sodium nitrate - Google Patents
A kind of method using core grade ZrO 2 production waste discharge production sodium nitrate Download PDFInfo
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- CN107934997A CN107934997A CN201711363820.7A CN201711363820A CN107934997A CN 107934997 A CN107934997 A CN 107934997A CN 201711363820 A CN201711363820 A CN 201711363820A CN 107934997 A CN107934997 A CN 107934997A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention is to provide a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate.The raffinate water produced more than the organic phase acidifying that specially separation of zirconium and hafnium process in core grade ZrO 2 production process is produced after water and hafnium extracting and enriching is neutralized with caustic soda, filtering removes solid precipitation particle, gained filtrate and the precipitation waste liquid produced in zirconium oxide preparation section, as produce the feed liquid of sodium nitrate.Feed liquid is concentrated by evaporation into evaporator, and concentrate is crystallized into flash evaporation crystallizer, and magma is filtered through centrifuge, can obtain sodium nitrate product.The technological process is simple, and the utilization of resources is abundant, and cost is relatively low, waste liquid abatement amount more than 90%, realizes environmental-friendly, has obvious social benefit and economic benefit.
Description
Technical field
The invention belongs to extract and separate field, and in particular to one kind utilizes core grade ZrO 2 production waste discharge production nitre
The method of sour sodium.
Background technology
Separation of zirconium and hafnium is committed step in core grade ZrO 2 production process.Under single nitric acid system, with tricresyl phosphate fourth
Ester makees extractant, and sulfonated kerosene makees diluent, forms the organic phase of zirconium hafnium extract and separate.The organic phase is before extracting system is entered
Need to be acidified with 6mol/L dilute nitric acid solutions, that is, acidulant in advance, the aqueous solution part produced after acidifying returns to extraction system
Acidulant is prepared, a part is handled as acid waste liquid；The extraction stoste that raffinate after zirconium hafnium extract and separate is enriched with as hafnium, warp
Raffinate water is produced after P204 extractions, a raffinate water part returns to zirconium hafnium extract and separate extraction system and prepares extraction stoste, a part
As acid waste liquid processing；Strip liquor, that is, zirconium nitrate acyl solution after zirconium hafnium extract and separate is precipitated with caustic soda, the hydrogen of generation
Zirconia slurry passes through separation of solid and liquid, and filtrated stock is alkalescent waste liquid.
Above two acid waste liquid contains zirconium, hafnium and other metal cations, and 2.5~4.5mol/L of nitric acid, need to add lime
Breast be neutralized to pH6~9 could outer row, since waste liquid amount is big, acidity is high, and neutralisation treatment cost is higher, the nitric acid in waste liquid
Fail effective recycling；Contain sodium nitrate in alkaline waste liquor, directly outer row's wasting of resources is larger, it is difficult to embodies its social benefit
And economic benefit.
This method use caustic soda in core grade ZrO 2 production process separation of zirconium and hafnium produce organic phase acidifying more than water with
And the raffinate water produced after hafnium extracting and enriching is neutralized, control certain pH value, be filtered to remove precipitation, filtrate and with zirconium oxide system
The mother liquor of precipitation of ammonium produced in standby process, the feed liquid as production sodium nitrate.Feed liquid through evaporation and concentration and flash crystallization, then through from
Scheming is filtered, and can obtain sodium nitrate product, and nitric acid and sodium nitrate overall recovery can reach more than 80% in waste liquid, and waste liquid amount is reduced
More than 90%, there is obvious social benefit and economic benefit.
The content of the invention
It is an object of the invention to：A kind of side using core grade ZrO 2 production waste discharge production sodium nitrate is provided
Method.This method technological process is simple, and the utilization of resources is abundant, and cost is relatively low, waste liquid abatement amount more than 90%, realize it is environmental-friendly,
With obvious social benefit and economic benefit.
Technical scheme is as follows：
The remarkable result of the present invention is：Technological process is simple, and the utilization of resources is abundant, and cost is relatively low, waste liquid abatement amount
More than 90%, realize environmental-friendly, there is obvious social benefit and economic benefit.
Brief description of the drawings
Fig. 1 is the process flow chart that waste discharge production sodium nitrate is produced using core grade ZrO 2 of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment is to of the present invention a kind of useless using the production discharge of core grade ZrO 2
The method of aquatic production sodium nitrate is described in further detail.
The present invention is to be related to a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate.Specially will
Produced more than the organic phase acidifying that separation of zirconium and hafnium process produces in core grade ZrO 2 production process after water and hafnium extracting and enriching
Raffinate water is neutralized with caustic soda, and filtering removes solid precipitation particle, and gained filtrate is given up with the precipitation produced in zirconium oxide preparation section
Liquid, as produces the feed liquid of sodium nitrate.Feed liquid into evaporator be concentrated by evaporation, concentrate into flash evaporation crystallizer crystallize, magma pass through from
Scheming is filtered, and can obtain sodium nitrate product.
A kind of method using core grade ZrO 2 production waste discharge production sodium nitrate, it is characterised in that：The technique bag
Include following step：
(1), by core grade ZrO 2 production process separation of zirconium and hafnium produce organic phase acidifying more than water liquid caustic soda in and
Neutralized in groove under room temperature, control endpoint pH, filtered with accurate filter and remove solid slag, filtrate is as sodium nitrate material
Liquid.
(2), and, terminal is controlled during the raffinate water produced after hafnium extracting and enriching is carried out with liquid caustic soda in neutralization chamber under room temperature
PH value, is filtered with accurate filter and removes the solid slags such as zirconium hydroxide, hafnium hydroxide, filtrate is as sodium nitrate feed liquid.
(3), the strip liquor after zirconium hafnium extract and separate, that is, zirconium nitrate acyl solution is precipitated with caustic soda, the zirconium hydroxide of generation
Slurry passes through separation of solid and liquid, and filtrate is as sodium nitrate feed liquid.
(4), sodium nitrate feed liquid is delivered to preheater with pump, and feed liquid preheating enters evaporator after reaching certain temperature, carries out
Be concentrated by evaporation, concentrate to flash crystallization system, carries out flash crystallization with pump input, crystalline particle enter under the effect of gravity from
Scheming is separated, and separated mother liquor goes neutralization chamber to recycle, and nitric acid sodium crystal is as product.
In the process of the present invention, 3.5~4.5mol/L of water concentration of nitric acid more than step (1) the organic phase acidifying；
Endpoint pH is 8~8.5.
In the process of the present invention, step (2) 3~4.5mol/L of the raffinate water concentration of nitric acid；Endpoint pH is 8
~8.5.
In the process of the present invention, the precipitation control ph of caustic soda described in step (3) is 8~8.5, nitric acid in filtrate
Na concn is 14%~25%.
In the process of the present invention, sodium nitrate concentration 10%~20% in feed liquid described in step (4), feed liquid preheating
Temperature is 80~85 DEG C；Sodium nitrate concentration is 55%~65% in concentrate；60~65 DEG C of flash crystallization temperature, flash crystallization pressure
10~15Kpa of power；Sodium nitrate product water content is less than 2%, and product meets GBT4533-2002 industrial sodium nitrate qualification quality
Standard.
Embodiment 1
(1), the 1m for producing separation of zirconium and hafnium in core grade ZrO 2 production process3Water is transported to pump more than organic phase acidifying
Neutralization chamber, sampling analysis concentration of nitric acid are 3.5mol/L；And, terminal is controlled in being carried out with 20% liquid caustic soda in neutralization chamber under room temperature
PH value is 8, is filtered with accurate filter, obtains wet filter residue 0.78kg, filtrate 1.6m3, analysis filtrate sodium nitrate concentration 15.62%,
The raw material that can be produced as sodium nitrate.
(2), the 1m that will be produced after hafnium extracting and enriching3Raffinate water is transported to neutralization chamber with pump, and sampling analysis concentration of nitric acid is
2.5mol/L；And, it is 8.0 to control endpoint pH, with accurate filter mistake in being carried out with 20% liquid caustic soda in neutralization chamber under room temperature
Filter, obtains the wet slag 1.1kg, filtrate 1.45m such as zirconium hydroxide, hafnium hydroxide3, analysis filtrate sodium nitrate concentration 12.38% can conduct
The raw material of sodium nitrate production.
(3), by the 1m after zirconium hafnium extract and separate3Strip liquor, that is, zirconium nitrate acyl solution is precipitated with 20% caustic soda, precipitation
Endpoint pH 8.0, the zirconium hydroxide slurry of generation pass through separation of solid and liquid, and solid goes dry, calcining after washing, prepares core level
Zirconium dioxide, filtrate 1.33m3, analysis filtrate sodium nitrate concentration 14.01%, the raw material that can be produced as sodium nitrate.
(4), by the feed liquid 20m of nitric acid sodium content 15%3With pump according to 850kg/h flows continuous conveying to preheater, material
Liquid enters evaporator after preheating 80 DEG C, is evaporated concentration, with pump input extremely sudden strain of a muscle after sodium nitrate concentration reaches 55% in concentrate
Steam crystal system, carry out flash crystallization, flash crystallization temperature 60 C, flash crystallization pressure 10Kpa, with flash distillation it is continuous into
OK, crystalline particle is separated into centrifuge under the effect of gravity, and separated mother liquor goes neutralization chamber to recycle, and is made aqueous
Sodium nitrate 2835kg of the amount less than 2%.
Embodiment 2
1), the 1m for producing separation of zirconium and hafnium in core grade ZrO 2 production process3Water is transported to pump more than organic phase acidifying
Neutralization chamber, sampling analysis concentration of nitric acid are 4.0mol/L；And, terminal is controlled in being carried out with 20% liquid caustic soda in neutralization chamber under room temperature
PH value is 8.5, is filtered with accurate filter, obtains wet filter residue 0.95kg, filtrate 1.68m3, analyze filtrate sodium nitrate concentration
18.35%, the raw material that can be produced as sodium nitrate.
(2), the 1m that will be produced after hafnium extracting and enriching3Raffinate water is transported to neutralization chamber with pump, and sampling analysis concentration of nitric acid is
4mol/L；And, it is 8.2 to control endpoint pH, is filtered with accurate filter in being carried out with 20% liquid caustic soda in neutralization chamber under room temperature,
Obtain the wet slag 1.1kg, filtrate 1.67m such as zirconium hydroxide, hafnium hydroxide3, analysis filtrate sodium nitrate concentration 16.93%, can be used as nitre
The raw material of sour sodium production.
(3), by the 1m after zirconium hafnium extract and separate3Strip liquor, that is, zirconium nitrate acyl solution is precipitated with 20% caustic soda, precipitation
Endpoint pH 8.2, the zirconium hydroxide slurry of generation pass through separation of solid and liquid, and solid goes dry, calcining after washing, prepares core level
Zirconium dioxide, filtrate 1.33m3, analysis filtrate sodium nitrate concentration 14.35%, the raw material that can be produced as sodium nitrate.
(4), by the feed liquid 20m of nitric acid sodium content 16.5%3With pump according to 850kg/h flows continuous conveying to preheater,
Feed liquid enters evaporator after preheating 85 DEG C, is evaporated concentration, is inputted extremely after sodium nitrate concentration reaches 60% in concentrate with pumping
Flash crystallization system, carry out flash crystallization, flash crystallization temperature 60 C, flash crystallization pressure 15Kpa, with flash distillation it is continuous into
OK, crystalline particle is separated into centrifuge under the effect of gravity, and separated mother liquor goes neutralization chamber to recycle, and is made aqueous
Sodium nitrate 3206kg of the amount less than 2%.
Embodiment 3
1), the 1m for producing separation of zirconium and hafnium in core grade ZrO 2 production process3Water is transported to pump more than organic phase acidifying
Neutralization chamber, sampling analysis concentration of nitric acid are 4.5mol/L；And, terminal is controlled in being carried out with 20% liquid caustic soda in neutralization chamber under room temperature
PH value is 8.3, is filtered with accurate filter, obtains wet filter residue 0.78kg, filtrate 1.71m3, analyze filtrate sodium nitrate concentration
18.15%, the raw material that can be produced as sodium nitrate.
(2), the 1m that will be produced after hafnium extracting and enriching3Raffinate water is transported to neutralization chamber with pump, and sampling analysis concentration of nitric acid is
4.5mol/L；And, it is 8.5 to control endpoint pH, with accurate filter mistake in being carried out with 20% liquid caustic soda in neutralization chamber under room temperature
Filter, obtains the wet slag 1.45kg, filtrate 1.8m such as zirconium hydroxide, hafnium hydroxide3, analysis filtrate sodium nitrate concentration 15.18% can conduct
The raw material of sodium nitrate production.
(3), by the 1m after zirconium hafnium extract and separate3Strip liquor, that is, zirconium nitrate acyl solution is precipitated with 20% caustic soda, precipitation
Endpoint pH 8.5, the zirconium hydroxide slurry of generation pass through separation of solid and liquid, and solid goes dry, calcining after washing, prepares core level
Zirconium dioxide, filtrate 1.35m3, analysis filtrate sodium nitrate concentration 14.65%, the raw material that can be produced as sodium nitrate.
(4), by the feed liquid 20m of nitric acid sodium content 17%3With pump according to 850kg/h flows continuous conveying to preheater, material
Liquid enters evaporator after preheating 85 DEG C, is evaporated concentration, with pump input extremely sudden strain of a muscle after sodium nitrate concentration reaches 55% in concentrate
Steam crystal system, carry out flash crystallization, 62 DEG C of flash crystallization temperature, flash crystallization pressure 12Kpa, with flash distillation it is continuous into
OK, crystalline particle is separated into centrifuge under the effect of gravity, and separated mother liquor goes neutralization chamber to recycle, and is made aqueous
Sodium nitrate 3335kg of the amount less than 2%.
Embodiment 4
1), the 1m for producing separation of zirconium and hafnium in core grade ZrO 2 production process3Water is transported to pump more than organic phase acidifying
Neutralization chamber, sampling analysis concentration of nitric acid are 4.5mol/L；And, terminal is controlled in being carried out with 20% liquid caustic soda in neutralization chamber under room temperature
PH value is 8, is filtered with accurate filter, obtains wet filter residue 0.75kg, filtrate 1.68m3, analysis filtrate sodium nitrate concentration 19.06%,
The raw material that can be produced as sodium nitrate.
(2), the 1m that will be produced after hafnium extracting and enriching3Raffinate water is transported to neutralization chamber with pump, and sampling analysis concentration of nitric acid is
4.3mol/L；And, it is 8 to control endpoint pH, is filtered with accurate filter in being carried out with 20% liquid caustic soda in neutralization chamber under room temperature,
Obtain the wet slag 1.26kg, filtrate 1.61m such as zirconium hydroxide, hafnium hydroxide3, analysis filtrate sodium nitrate concentration 16.86%, can be used as nitre
The raw material of sour sodium production.
(3), by the 1m after zirconium hafnium extract and separate3Strip liquor, that is, zirconium nitrate acyl solution is precipitated with 20% caustic soda, precipitation
Endpoint pH 8.3, the zirconium hydroxide slurry of generation pass through separation of solid and liquid, and solid goes dry, calcining after washing, prepares core level
Zirconium dioxide, filtrate 1.1m3, analysis filtrate sodium nitrate concentration 23%, the raw material that can be produced as sodium nitrate.
(4), by the feed liquid 20m of nitric acid sodium content 20%3With pump according to 850kg/h flows continuous conveying to preheater, material
Liquid enters evaporator after preheating 80 DEG C, is evaporated concentration, with pump input extremely sudden strain of a muscle after sodium nitrate concentration reaches 60% in concentrate
Steam crystal system, carry out flash crystallization, 65 DEG C of flash crystallization temperature, flash crystallization pressure 10Kpa, with flash distillation it is continuous into
OK, crystalline particle is separated into centrifuge under the effect of gravity, and separated mother liquor goes neutralization chamber to recycle, and is made aqueous
Sodium nitrate 3910kg of the amount less than 2%.
Claims (10)
- A kind of 1. method using core grade ZrO 2 production waste discharge production sodium nitrate, it is characterised in that：Including following step Suddenly：(1) water NaOH solution is in neutralization chamber more than the organic phase acidifying produced separation of zirconium and hafnium in core grade ZrO 2 production process Neutralized under middle room temperature, control endpoint pH, filtered with accurate filter and remove solid slag, filtrate is as sodium nitrate feed liquid；(2) and, terminal is controlled during the raffinate water produced after hafnium extracting and enriching is carried out with NaOH solution in neutralization chamber under room temperature PH value, is filtered with accurate filter and removes solid slag, filtrate is as sodium nitrate feed liquid；(3) strip liquor after zirconium hafnium extract and separate is precipitated with NaOH solids, and the zirconium hydroxide slurry of generation is by solid-liquid point From filtrate is as sodium nitrate feed liquid；(4) the sodium nitrate feed liquid obtained in step (1), (2) and (3) is delivered to preheater with pump, feed liquid is carried out preheating reaches Entering evaporator after to certain temperature, be evaporated concentration, concentrate is delivered to flash crystallization system with pump and carries out flash crystallization, Crystalline particle is separated into centrifuge under the effect of gravity, obtains nitric acid sodium crystal, and separated mother liquor is delivered to neutralization chamber Recycle.
- 2. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：3.5~4.5mol/L of water concentration of nitric acid more than organic phase acidifying described in step (1).
- 3. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：Endpoint pH described in step (1) is 8~8.5.
- 4. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：2.5~4.5mol/L of raffinate water concentration of nitric acid described in step (2).
- 5. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：Endpoint pH described in step (2) is 8~8.5.
- 6. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：The precipitation control ph of caustic soda described in step (3) is 8~8.5.
- 7. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：Sodium nitrate concentration is 14%~25% in filtrate described in step (3).
- 8. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：Feed liquid preheating temperature described in step (4) is 80~85 DEG C.
- 9. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：Sodium nitrate concentration is 55%~65% in concentrate described in step (4).
- 10. a kind of method using core grade ZrO 2 production waste discharge production sodium nitrate as claimed in claim 1, its feature It is：60~65 DEG C of flash crystallization temperature described in step (4), 10~15Kpa of flash crystallization pressure；Sodium nitrate product is aqueous Amount is less than 2%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112573571A (en) * | 2020-11-20 | 2021-03-30 | 中核二七二铀业有限责任公司 | Method for preparing hafnium dioxide from sodium hafnocenate |
| CN112723413A (en) * | 2020-11-20 | 2021-04-30 | 中核二七二铀业有限责任公司 | Production method of nuclear-grade zirconium dioxide |
| CN114275748A (en) * | 2021-12-31 | 2022-04-05 | 中核二七二铀业有限责任公司 | Method for producing nitric acid and sodium nitrate by using wastewater discharged from nuclear-grade hafnium oxide production |
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| KR20030086031A (en) * | 2002-05-03 | 2003-11-07 | 윤취주 | Method for Preparing Sodium Nitrate Using Waste Nitric Acid |
| CN101070168A (en) * | 2007-06-26 | 2007-11-14 | 中国中轻国际工程有限公司 | Method for producing sodium nitrate |
| CN107010771A (en) * | 2017-04-10 | 2017-08-04 | 湖北振华化学股份有限公司 | Medium chrome yellow production technology Sewage treatment Application way |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030086031A (en) * | 2002-05-03 | 2003-11-07 | 윤취주 | Method for Preparing Sodium Nitrate Using Waste Nitric Acid |
| CN101070168A (en) * | 2007-06-26 | 2007-11-14 | 中国中轻国际工程有限公司 | Method for producing sodium nitrate |
| CN107010771A (en) * | 2017-04-10 | 2017-08-04 | 湖北振华化学股份有限公司 | Medium chrome yellow production technology Sewage treatment Application way |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112573571A (en) * | 2020-11-20 | 2021-03-30 | 中核二七二铀业有限责任公司 | Method for preparing hafnium dioxide from sodium hafnocenate |
| CN112723413A (en) * | 2020-11-20 | 2021-04-30 | 中核二七二铀业有限责任公司 | Production method of nuclear-grade zirconium dioxide |
| CN114275748A (en) * | 2021-12-31 | 2022-04-05 | 中核二七二铀业有限责任公司 | Method for producing nitric acid and sodium nitrate by using wastewater discharged from nuclear-grade hafnium oxide production |
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